metal-organic compounds
Data collection
reports the structure of one such complex, (I), determined by
single-crystal X-ray diffraction analysis.
Bruker SMART CCD area-detector
diffractometer
' and ! scans
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
Tmin = 0.728, Tmax = 0.834
13 305 measured re¯ections
6871 independent re¯ections
5931 re¯ections with I > 2ꢆ(I)
Rint = 0.032
ꢅmax = 28.4ꢀ
Each La3+ ion is coordinated by seven O atoms and one N
atom from a 4,40-bipyridine molecule, where six of the O
atoms (O1, O1A, O2A, O3, O4A and O5) are from ®ve
different 2-¯uorobenzoate groups and the seventh (O7) is
from a water molecule (Fig. 1). The carboxylate groups adopt
three coordination modes, viz. monodentate, bidentate brid-
ging and bidentate chelating. Two La3+ ions form a dimeric
molecule, with four bridging carboxylate groups. The O5/C15/
O6 carboxylate groups are monodentate, with one atom (O5)
coordinated to the La3+ ion. The O3/C8/O4 groups are brid-
ging, with the two O atoms coordinating to different La3+ ions.
The O1/C1/O2 groups are in the chelating-bridging mode, in
which two O atoms chelate one La3+ ion and one of the O
atoms is linked to the other La3+ ion. The LaÐOcarboxy
distances in the title complex range from 2.471 (2) to
h = 12 ! 13
k = 15 ! 16
l = 17 ! 16
Re®nement
Re®nement on F2
R[F2 > 2ꢆ(F2)] = 0.030
wR(F2) = 0.080
S = 1.08
6871 re¯ections
w = 1/[ꢆ2(F2o) + (0.0392P)2]
where P = (F2o+2Fc2)/3
(Á/ꢆ)max = 0.002
3
Ê
Áꢇmax = 0.77 e A
3
Ê
1.02 e A
Áꢇmin
=
397 parameters
H-atom parameters constrained
Ê
Ê
2.942 (3) A (mean 2.569 A) and the OÐLaÐO angles range
from 71.51 (9) to 143.64 (8)ꢀ. One N atom from a 4,40-bi-
pyridine molecule is coordinated to the La3+ ion, the La1ÐN1
Table 1
Hydrogen-bonding geometry (A, ).
ꢀ
Ê
DÐHÁ Á ÁA
DÐH
HÁ Á ÁA
DÁ Á ÁA
DÐHÁ Á ÁA
Ê
bond distance being 2.852 (3) A; this conformation contrasts
with that in the [{Eu(DBM)3}2(ꢀ-4,40-bipy)] complex (DBM is
dibenzoylmethane), in which two N atoms from a 4,40-bi-
pyridine molecule link two Eu3+ ions, resulting in an in®nite
polymeric chain (Wang et al., 1995). Each La3+ ion is also
coordinated by a water molecule, the LaÐOwater bond
O7ÐH7AÁ Á ÁN2i
O7ÐH7BÁ Á ÁO5ii
C5ÐH5Á Á ÁF3iii
0.85
0.85
0.93
0.93
2.02
2.50
2.52
2.44
2.855 (4)
3.158 (4)
3.379 (5)
2.950 (4)
168
135
153
115
C26ÐH26Á Á ÁO2iv
Symmetry codes: (i) 1 x; 1 y; 1 z; (ii) x; 1 y; 1 z; (iii) x; 2 y; 1 z; (iv)
1
x; 1 y; 1 z.
Ê
distance being 2.572 (3) A.
Hydrogen bonds (Table 1) exist between two dimeric mol-
ecules, involving the non-coordinated N atom of the 4,40-
bipyridine group of one dimeric molecule and the H atom
of the coordinated water molecule of another dimer
H atoms were placed at calculated positions, with CÐH distances
Ê
of 0.93 A and water OÐH distances of 0.85 A.
Ê
ꢀ
Data collection: SMART (Bruker, 1997); cell re®nement: SMART;
data reduction: SAINT (Bruker, 1997); program(s) used to solve
structure: SHELXS97 (Sheldrick, 1990); program(s) used to re®ne
structure: SHELXL97 (Sheldrick, 1997); molecular graphics:
SHELXTL (Bruker, 1998); software used to prepare material for
publication: SHELXTL.
Ê
(HÁ Á ÁN = 2.02 A and OÐHÁ Á ÁN = 168 ; symmetry code: 1 + x,
1 + y, 1 + z). An in®nite one-dimensional dimeric supramo-
lecular chain is formed, linked by the hydrogen bonds.
Experimental
LaCl3Á6H2O (0.5 mmol), 2-¯uorobenzoic acid (1.5 mmol) and 4,40-
bipyridine (0.5 mmol) were dissolved separately in appropriate
amounts of ethanol. The ethanol solution of 2-¯uorobenzoic acid was
adjusted to pH 6±7 with an aqueous solution of NaOH (2 mol dm 3),
and then the ethanol solutions of 4,40-bipyridine and LaCl3 were
added dropwise. The mixture was heated under re¯ux with stirring
for 2 h and the resulting white minor precipitate was ®ltered off.
Single crystals were obtained from the mother liquor after it had been
left to stand for one month at room temperature.
The authors are grateful to the Natural Science Foundation
of Beijing (grant No. 2022007), SRF for ROCS, SEM, and the
Beijing Foundation of Science and Technology.
Supplementary data for this paper are available from the IUCr electronic
archives (Reference: AV1158). Services for accessing these data are
described at the back of the journal.
Crystal data
[La(C7H4FO2)6(C10H8N2)2(H2O)2]
Mr = 730.42
Triclinic, P1
Z = 2
Dx = 1.698 Mg m
Mo Kꢂ radiation
References
3
Bruker (1997). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin,
USA.
Bruker (1998). SHELXTL. Bruker AXS Inc., Madison, Wisconsin, USA.
Sheldrick, G. M. (1990). Acta Cryst. A46, 467±473.
Sheldrick, G. M. (1996). SADABS. University of GoÈttingen, Germany.
Sheldrick, G. M. (1997). SHELXL97. University of Gottingen, Germany.
Wang, M.-Z., Jin, L.-P., Wang, Z.-M., Cai, G.-L. & Zhang, J.-H. (1995). Sci.
China Ser. B, 38, 1061.
Ê
a = 9.746 (5) A
Cell parameters from 986
re¯ections
Ê
b = 12.780 (7) A
c = 13.315 (7) A
ꢅ = 3.2±28.0ꢀ
ꢀ = 1.57 mm
T = 293 (2) K
Ê
1
ꢂ = 113.132 (9)ꢀ
ꢃ = 104.763 (9)ꢀ
ꢄ = 96.916 (9)ꢀ
È
Prism, white
0.20 Â 0.18 Â 0.12 mm
3
Ê
V = 1428.6 (13) A
ꢁ
Acta Cryst. (2004). C60, m110±m111
Li, Zou and Song
[La(C7H4FO2)6(C10H8N2)2(H2O)2] m111
Li, Xia
